公开(公告)号：US20080214836A1

公开(公告)日：2008-09-04

申请号：US11472024

申请日：2006-06-21

Applicant: Eric Lacroix ,  Serge Hub ,  Wolfgang Holderich ,  Wilm Eickelberg ,  Francois Fajula ,  Francesco DiRenzo ,  Markus Brandhorst

Inventor： Eric Lacroix ,  Serge Hub ,  Wolfgang Holderich ,  Wilm Eickelberg ,  Francois Fajula ,  Francesco DiRenzo ,  Markus Brandhorst

IPC: C07D207/12

CPC classification number: C07D201/04

Abstract: The present invention relates to a process for the preparation of lauryllactam in which a Beckmann rearrangement of cyclododecanone oxime is carried out. Said process is carried out in the gas phase at a temperature of between 180 and 450° C. in the presence of a microporous material having a three-dimensional inorganic main structure composed of tetrahedra connected via a common edge, called zeolite.

Abstract translation: 本发明涉及一种制备十二烷基内酰胺的方法，其中进行了环十二烷酮肟的贝克曼重排。 所述方法在气相中，在具有三维无机主体结构的微孔材料的存在下，在180-450℃的温度下进行，所述三维无机主体结构由通过共同边缘连接的四面体称为沸石。

公开(公告)号：US20080033168A1

公开(公告)日：2008-02-07

申请号：US11822141

申请日：2007-07-02

Applicant: Keisuke Sugita ,  Masaru Kitamura

Inventor： Keisuke Sugita ,  Masaru Kitamura

IPC: C07D201/04 ,  B01J38/70

CPC classification number: B01J29/90 ,  B01J38/66 ,  B01J2229/32 ,  C07D201/04 ,  Y02P20/52 ,  Y02P20/584

Abstract: The present invention provides a process for regenerating a catalyst for producing e-caprolactam comprising the steps of adsorbing a silicon compound on a zeolite catalyst that had been used for a Beckmann rearrangement reaction of cyclohexanone oxime and contacting the catalyst with an aqueous solution containing a compound selected from a quaternary ammonium compound, lower alkylamines and ammonia. The present invention also provides a process for producing e-caprolactam comprising subjecting cyclohexanone oxime to the Beckmann rearrangement reaction in the presence of the catalyst thus regenerated.

Abstract translation: 本发明提供了一种用于再生生产ε-己内酰胺的催化剂的方法，包括以下步骤：将硅化合物吸附在已经用于环己酮肟的贝克曼重排反应的沸石催化剂上，并使催化剂与含有化合物的水溶液接触 选自季铵化合物，低级烷基胺和氨。 本发明还提供一种生产ε-己内酰胺的方法，其包括在由此再生的催化剂存在下使环己酮肟进行贝克曼重排反应。

公开(公告)号：US20070083043A1

公开(公告)日：2007-04-12

申请号：US10557771

申请日：2004-05-17

Applicant: Petrus Jozef Thomissen ,  Joannes Albertus Lemmens ,  Theodorus Smeets

Inventor： Petrus Jozef Thomissen ,  Joannes Albertus Lemmens ,  Theodorus Smeets

IPC: C07D201/04

CPC classification number: B01F5/0428 ,  B01F5/0415 ,  B01J19/26 ,  B01J2219/00164 ,  C07D201/04

Abstract: The invention relates to a process for preparing caprolactam by Beckmann rearrangement of cyclohexanone oxime by feeding cyclohexanone oxime to a reaction mixture comprising (i) sulfuric acid (ii) S03 and (iii) caprolactam, wherein the S03 content of the reaction mixture is between 9 and 20 wt. % and the molar ratio M of the reaction mixture defined as (nSO3+nH2SO4)/ncap is between 1 and 1.4, wherein nSO3=quantity of SO3 in reaction mixture, in mol nH2SO4=quantity of H2SO4 in reaction mixture, in mol ncap=quantity of caprolactam in reaction mixture, in mol.

Abstract translation: 本发明涉及通过将环己酮肟进料到包含（i）硫酸（ⅱ）S 3 H 3和（ⅲ）己内酰胺的反应混合物中的环己酮肟贝克曼重排制备己内酰胺的方法，其中S 0 反应混合物的含量为9至20重量％。 ％，反应混合物的摩尔比M定义为（n SO 3 H + H 2 SO 4）/ n帽帽，为1至1.4，其中 反应混合物中的SO 3的量为N 2 H 2 SO 4的量

公开(公告)号：US07189845B2

公开(公告)日：2007-03-13

申请号：US11088874

申请日：2005-03-25

Applicant: Keisuke Sugita ,  Masaru Kitamura ,  Masahiro Hoshino

Inventor： Keisuke Sugita ,  Masaru Kitamura ,  Masahiro Hoshino

IPC: C07D201/04

CPC classification number: C07D201/04 ,  B01J29/90 ,  B01J38/12 ,  Y02P20/52 ,  Y02P20/584

Abstract: The invention provides a method for producing ε-caprolactam comprising the steps of: a reaction process which subjects cyclohexanone oxime to a Beckmann rearrangement reaction in the presence of a solid catalyst; and a catalyst regeneration process which regenerates the solid catalyst used in the reaction process by heat treatment under an atmosphere comprising an oxygen-containing gas, wherein the solid catalyst heat-treated in the catalyst regeneration process is used in the reaction process, the carbon contents in the solid catalyst in the reaction process and the catalyst regeneration process are maintained in a range of 0.5 to 2% by weight, and the nitrogen contents in the solid catalyst in the reaction process and the catalyst regeneration process are maintained in a range of 0.01 to 0.2% by weight.According to the invention, ε-caprolactam can be produced in a high production yield for a long period of time by enhancing persistence of the catalytic activity for producing ε-caprolactam.

Abstract translation: 本发明提供了一种生产ε-己内酰胺的方法，包括以下步骤：在固体催化剂存在下将环己酮肟与贝克曼重排反应相对应的反应过程; 以及催化剂再生方法，其通过在包含含氧气体的气氛下进行热处理来再生反应过程中使用的固体催化剂，其中在反应过程中使用在催化剂再生过程中热处理的固体催化剂，碳含量 在反应过程中的固体催化剂和催化剂再生过程保持在0.5〜2重量％的范围内，并且在反应过程和催化剂再生过程中固体催化剂中的氮含量保持在0.01 至0.2重量％。 根据本发明，ε-己内酰胺可以通过增加用于生产ε-己内酰胺的催化活性的持久性，以高生产率长时间生产。

公开(公告)号：US07084269B2

公开(公告)日：2006-08-01

申请号：US10471750

申请日：2002-03-05

Applicant: Kiyotaka Hatakeda ,  Osamu Sato ,  Yutaka Ikushima ,  Kazuo Torii

Inventor： Kiyotaka Hatakeda ,  Osamu Sato ,  Yutaka Ikushima ,  Kazuo Torii

IPC: C07D201/04

CPC classification number: C07D201/04

Abstract: It is an object of the present invention to provide an efficient method of continuously producing a lactam in high-temperature high-pressure water, and the present invention relates to a method of producing a lactam characterized by efficiently synthesizing the lactam while suppressing oxime hydrolysis by introducing an oxime as a reaction substrate and an acid into a reaction zone through which high-temperature high-pressure water is flowing, or introducing an oxime into flowing high-temperature high-pressure water containing an acid, thus raising the temperature of the reaction substrate to put the reaction substrate into a prescribed high-temperature high-pressure state within a short time and subjecting the reaction substrate to reaction; through the method, the lactam can be efficiently and continuously synthesized at a high rate from the oxime using an acid catalyst in water at a high temperature of at least 250° C. and a high pressure of at least 15 MPa.

Abstract translation: 本发明的目的是提供一种在高温高压水中连续生产内酰胺的有效方法，本发明涉及一种制备内酰胺的方法，其特征在于在抑制肟水解的同时有效地合成内酰胺 将肟作为反应基质和酸引入高温高压水流过的反应区，或将肟引入流入含有酸的高温高压水中，从而提高反应温度 将反应基材在短时间内放入规定的高温高压状态，使反应基板反应; 通过该方法，可以使用酸催化剂在高温下在高温至少250℃，高压至少15MPa的水中，以高速从肟高效连续地合成内酰胺。

公开(公告)号：US07045622B2

公开(公告)日：2006-05-16

申请号：US10469533

申请日：2001-03-23

Applicant: Kiyotaka Hatakeda ,  Osamu Sato ,  Yutaka Ikushima ,  Kazuo Torii

Inventor： Kiyotaka Hatakeda ,  Osamu Sato ,  Yutaka Ikushima ,  Kazuo Torii

IPC: C07D201/04 ,  C07D223/10

CPC classification number: C07D201/06 ,  C07D201/04 ,  C07D223/10

Abstract: It is an object of the present invention to provide a method of continuously producing a lactam in high-temperature high-pressure water, and the present invention relates to a method for producing a lactam characterized by selectively synthesizing the lactam without bringing about hydrolysis by introducing an oxime into flowing high-temperature high-pressure water, wherein the lactam is continuously synthesized at a high rate from the oxime in water at a high temperature of at least 250° C. and a high pressure of at least 12 MPa.

Abstract translation: 本发明的目的是提供一种在高温高压水中连续生产内酰胺的方法，本发明涉及一种制备内酰胺的方法，其特征在于，通过引入不引起水解而选择性合成内酰胺 将肟流入高温高压水中，其中在至少250℃的高温和至少12MPa的高压下，从肟在水中以高速连续合成内酰胺。

公开(公告)号：US20060094873A1

公开(公告)日：2006-05-04

申请号：US11311604

申请日：2005-12-19

Applicant: Alan Levy ,  Gregory Cleotelis ,  James Sawyer ,  Nolan Henrich ,  Mohammed Loya ,  Matthew Warren ,  Gregory Moore

Inventor： Alan Levy ,  Gregory Cleotelis ,  James Sawyer ,  Nolan Henrich ,  Mohammed Loya ,  Matthew Warren ,  Gregory Moore

IPC: C07D201/04

CPC classification number: C07D201/04

Abstract: Methods are disclosed of producing and purifying at least one amide. In accordance with one of the methods disclosed herein, the at least one amide is produced by providing an organic liquid comprising at least one oxime, providing at least one catalyst, adding the at least one catalyst to the organic liquid to form a rearrangement mass, wherein the rearrangement mass comprises at least one amide, at least one impurity, and the at least one catalyst, and heating the rearrangement mass to a temperature of at least about 115° C. for a period of time in order to sulfonate, break down and/or reduce the concentration of some of the at least one impurity in the rearrangement mass.

公开(公告)号：US20050245740A1

公开(公告)日：2005-11-03

申请号：US11088874

申请日：2005-03-25

Applicant: Keisuke Sugita ,  Masaru Kitamura ,  Masahiro Hoshino

Inventor： Keisuke Sugita ,  Masaru Kitamura ,  Masahiro Hoshino

IPC: C07D223/10 ,  B01J29/90 ,  B01J38/12 ,  C07B61/00 ,  C07D201/04 ,  B01J20/34

CPC classification number: C07D201/04 ,  B01J29/90 ,  B01J38/12 ,  Y02P20/52 ,  Y02P20/584

Abstract: The invention provides a method for producing ε-caprolactam comprising the steps of: a reaction process which subjects cyclohexanone oxime to a Beckmann rearrangement reaction in the presence of a solid catalyst; and a catalyst regeneration process which regenerates the solid catalyst used in the reaction process by heat treatment under an atmosphere comprising an oxygen-containing gas, wherein the solid catalyst heat-treated in the catalyst regeneration process is used in the reaction process, the carbon contents in the solid catalyst in the reaction process and the catalyst regeneration process are maintained in a range of 0.5 to 2% by weight, and the nitrogen contents in the solid catalyst in the reaction process and the catalyst regeneration process are maintained in a range of 0.01 to 0.2% by weight. According to the invention, ε-caprolactam can be produced in a high production yield for a long period of time by enhancing persistence of the catalytic activity for producing ε-caprolactam.

Abstract translation: 本发明提供了一种生产ε-己内酰胺的方法，包括以下步骤：在固体催化剂存在下将环己酮肟与贝克曼重排反应相对应的反应过程; 以及催化剂再生方法，其通过在包含含氧气体的气氛下进行热处理来再生反应过程中使用的固体催化剂，其中在反应过程中使用在催化剂再生过程中热处理的固体催化剂，碳含量 在反应过程中的固体催化剂和催化剂再生过程保持在0.5〜2重量％的范围内，并且在反应过程和催化剂再生过程中固体催化剂中的氮含量保持在0.01 至0.2重量％。 根据本发明，ε-己内酰胺可以通过增加用于生产ε-己内酰胺的催化活性的持久性，以高生产率长时间生产。

公开(公告)号：US20050182254A1

公开(公告)日：2005-08-18

申请号：US11055101

申请日：2005-02-11

Applicant: Keisuke Sugita ,  Masaru Kitamura ,  Masahiro Hoshino

Inventor： Keisuke Sugita ,  Masaru Kitamura ,  Masahiro Hoshino

IPC: C07D223/10 ,  B01J29/035 ,  B01J29/90 ,  B01J38/06 ,  B01J38/08 ,  B01J38/12 ,  B01J38/18 ,  B01J38/62 ,  B01J38/66 ,  C07B61/00 ,  C07D201/04 ,  C07D201/14 ,  B01J38/04

CPC classification number: B01J38/08 ,  B01J29/90 ,  B01J38/12 ,  B01J38/66 ,  C07D201/04 ,  Y02P20/52 ,  Y02P20/584

Abstract: A method for producing ε-caprolactam and a method for reactivating a zeolite catalyst for the production are provided. In the reactivation step, a zeolite catalyst is allowed to contact a gas containing a carboxylic acid, water and a compound selected from ammonia and amines. In accordance with the present invention, the catalytic activities of a zeolite catalyst used for the Beckmann rearrangement reaction of cyclohexanone oxime can be effectively restored. Consequently, ε-caprolactam may be produced with a high production yield for a long period of time by reusing the catalyst by the method described above.

Abstract translation: 提供了制备ε-己内酰胺的方法和用于再生催化剂的方法。 在再活化步骤中，使沸石催化剂与含有羧酸，水和选自氨和胺的化合物的气体接触。 根据本发明，可以有效地恢复用于环己酮肟的贝克曼重排反应的沸石催化剂的催化活性。 因此，通过上述方法重新使用催化剂，可以长期生产ε-己内酰胺。

公开(公告)号：US20050010020A1

公开(公告)日：2005-01-13

申请号：US10883822

申请日：2004-07-06

Applicant: Masashi Yokota ,  Yoshinori Kobayashi ,  Masaru Kitamura

Inventor： Masashi Yokota ,  Yoshinori Kobayashi ,  Masaru Kitamura

IPC: C07D201/10 ,  C07D201/04 ,  C08G69/08 ,  C07D223/10 ,  C08G73/10

CPC classification number: C07D201/04 ,  Y02P20/52

Abstract: ε-Caprolactam is produced by the method comprising the step of introducing a gas comprising cyclohexanone oxime into a layer of solid catalyst particles through a plurality of holes of a gas diffusion plate so that the solid catalyst particles are brought into contact with the gas, while fluidizing the catalyst layer, wherein the holes have an average diameter of about 3 mm or smaller. In accordance with the production method, ε-caprolactam can be produced from a raw material gas comprising cyclohexanone oxime with a high conversion of cyclohexanone oxime and a high selectivity to ε-caprolactam.

Abstract translation: ε-己内酰胺通过包括以下步骤的方法制备：包括环己酮肟的气体通过气体扩散板的多个孔引入固体催化剂颗粒层中，使得固体催化剂颗粒与气体接触，同时 使催化剂层流化，其中孔的平均直径为约3mm或更小。 根据制造方法，ε-己内酰胺可以由包含环己酮肟的高转化率和对ε-己内酰胺的高选择性的环己酮肟的原料气体制备。